CN112619604A - 4A molecular sieve and preparation method thereof - Google Patents
4A molecular sieve and preparation method thereof Download PDFInfo
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/16—Alumino-silicates
- B01J20/18—Synthetic zeolitic molecular sieves
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- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
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Abstract
The application relates to the field of molecular sieves, and particularly discloses a 4A molecular sieve and a preparation method thereof. A4A molecular sieve comprises zeolite, binder, carbon black, fumed silica; the preparation method comprises the following steps: mixing zeolite, adhesive, carbon black and fumed silica to obtain a first mixture; adding the first mixture into a ball rolling machine for rolling balls, and simultaneously adding a binder into the first mixture in the ball rolling machine to obtain a first crude product; adding the screened first crude product into a rolling mill for rolling, and simultaneously adding silica sol into the first crude product in the rolling mill to obtain a second crude product; and drying, roasting and cooling the second crude product in sequence to obtain the 4A molecular sieve. The 4A molecular sieve can be used for adsorbing water, methanol, ethanol, hydrogen sulfide, sulfur dioxide, carbon dioxide, ethylene and propylene, and has the advantage of low abrasion rate.
Description
Technical Field
The application relates to the field of molecular sieves, in particular to a 4A molecular sieve and a preparation method thereof
Background
The 4A molecular sieve has a pore diameter of 4A, adsorbs water, methanol, ethanol, hydrogen sulfide, sulfur dioxide, carbon dioxide, ethylene and propylene, does not adsorb any molecules (including propane) with a diameter larger than 4A, and has a selective adsorption performance on water higher than that of any other molecules. Is one of the most industrially used molecular sieve varieties. It is mainly suitable for drying gas and liquid. Can adsorb H2O, NH3, H2S, CO2, SO2, CO, methyl chloride, methyl bromide, acetylene, ethane, ethylene, propylene and the like. It is widely used for drying petroleum gas, natural gas and the like in oil fields. It is also widely used for dehydration of ethanol.
The raw material composition of the 4A molecular sieve in the related art comprises zeolite and a binder.
When the 4A molecular sieve in the related technology is used, the abrasion rate is high, and further the service life is easy to be low.
Disclosure of Invention
In order to improve the abrasion rate of the molecular sieve, the application provides a 4A molecular sieve and a preparation method thereof.
In a first aspect, the present application provides a 4A molecular sieve, which adopts the following technical scheme:
A4A molecular sieve is prepared from the following raw materials in percentage by mass:
the zeolite is a 4A zeolite.
By adopting the technical scheme, because the carbon black and the fumed silica are added, the wear resistance of the 4A molecular sieve in the application is obviously improved, and the adsorption performance of the 4A molecular sieve in the application is improved due to the porous structure of the carbon black.
Preferably, the binder is one or two of attapulgite and kaolin.
Through adopting above-mentioned technical scheme, attapulgite not only has good cohesiveness, and has good stream ability concurrently, and the cohesiveness of kaolin is excellent, can make each component combination in the raw materials inseparabler, and then promotes the wear resistance of the 4A molecular sieve in this application.
Preferably, the adhesive consists of attapulgite and kaolin, the attapulgite accounts for 5-15% of the mass of the 4A molecular sieve, and the kaolin accounts for 5-15% of the mass of the 4A molecular sieve.
Through adopting above-mentioned technical scheme, add attapulgite and kaolin jointly, not only can promote the adhesion of each raw materials in the 4A molecular sieve in this application, and promoted the water absorption capacity of 4A molecular sieve in this application simultaneously.
Preferably, the mass percent of the carbon black is 3-5%.
By adopting the technical scheme, the abrasion rate of the 4A molecular sieve in the application can be reduced to 0.22-0.3%.
Preferably, the mass percent of the fumed silica is 12-16%.
By adopting the technical scheme, the abrasion rate of the 4A molecular sieve in the application can be reduced to 0.22-0.3%.
In a second aspect, the present application provides a method for preparing a 4A molecular sieve, which adopts the following technical scheme:
a preparation method of a 4A molecular sieve comprises the following steps:
(1) uniformly mixing zeolite, carbon black, fumed silica and an adhesive to obtain a first mixture;
(2) adding the mixture I in the step (1) into a ball rolling machine, spraying water on the surface of the mixture I, adding an adhesive, controlling the rotating speed of the ball rolling machine to be 50-150 r/min, rolling for 10-20 min, then spraying water again, adding the adhesive, and repeating the process until the particle size of material particles in the ball rolling machine reaches 2-2.5 mm, so as to obtain a first coarse product;
(3) screening the first crude product in the step (2);
(4) adding the first coarse product screened in the step (3) into a ball rolling machine, controlling the rotating speed of the ball rolling machine to be 30-120 r/min, rolling for 10-15 min, and spraying silica sol to the first coarse product while rolling the ball to obtain a second coarse product;
(5) putting the second crude product in the step (4) into a dryer to carry out five-stage continuous drying, wherein the temperature of the first-stage drying is controlled to be 60-80 ℃, the temperature of the second-stage drying is controlled to be 70-90 ℃, the temperature of the third-stage drying is controlled to be 80-100 ℃, the temperature of the fourth-stage drying is controlled to be 90-110 ℃, the temperature of the fifth-stage drying is controlled to be 100-120 ℃, and the water content of the second crude product after drying is controlled to be 30%;
(6) baking the second crude product dried in the step (5) in a rotary furnace, wherein the rotary furnace comprises six temperature zones, and the second crude product sequentially passes through a first temperature zone, a second temperature zone, a third temperature zone, a fourth temperature zone, a fifth temperature zone and a sixth temperature zone;
controlling the temperature of the first temperature zone to be 200-250 ℃, the temperature of the second temperature zone to be 250-300 ℃, the temperature of the third temperature zone to be 300-350 ℃, the temperature of the fourth temperature zone to be 400-450 ℃, the temperature of the fifth temperature zone to be 450-500 ℃, the temperature of the sixth temperature zone to be 500-550 ℃, and the total time of the second crude product passing through the six temperature zones to be 120-140 min, and finishing the baking operation to obtain a third crude product;
(7) and (4) screening the third crude product in the step (6), standing and cooling to obtain the 4A molecular sieve.
By adopting the technical scheme, the second crude product is dried by gradually heating for four times, so that the second crude product is difficult to crack due to the steep temperature rise; roast the second coarse product through six times temperature rise gradually for the second coarse product is difficult to the fracture when being roasted the design, and adopts the mode of being less than 600 ℃ of roasting for a long time, can avoid the carbon black to produce the burning, and through adding the silica sol, can further promote the wear resistance of the 4A molecular sieve in this application.
Preferably, the mass percentage of the added silica sol in the step (4) is 1-5%.
By adopting the technical scheme, the abrasion rate of the 4A molecular sieve in the application can be reduced to be less than 0.35%.
Preferably, the mass percentage of the added silica sol in the step (4) is 3-5%.
By adopting the technical scheme, the abrasion rate of the 4A molecular sieve in the application can be reduced to be less than 0.26%.
In summary, the present application has the following beneficial effects:
1. because the 4A molecular sieve is added with the carbon black and the fumed silica, the abrasion rate of the 4A molecular sieve is greatly reduced, and the water absorption performance of the 4A molecular sieve can be improved;
2. the carbon black is preferably added in an amount of 3-5% by mass, and in the range, the abrasion rate of the 4A molecular sieve can be reduced to 0.22-0.3%;
3. according to the method, the moisture of the 4A molecular sieve is reduced through the four-stage progressive drying and the six-stage progressive roasting, the molecular sieve can be shaped, and the probability that the 4A molecular sieve is cracked in the drying and roasting operation can be reduced.
Detailed Description
The present application will be described in further detail with reference to examples.
Raw material
Examples
Example 1
A4A molecular sieve is prepared from the following raw materials in percentage by mass:
the preparation method of the 4A molecular sieve comprises the following operation steps:
(1) uniformly mixing zeolite, carbon black, fumed silica and an adhesive to obtain a first mixture;
(2) adding the mixture I in the step (1) into a ball rolling machine, spraying water on the surface of the mixture I, adding an adhesive, controlling the rotating speed of the ball rolling machine to be 150r/min, rolling for 20min, then spraying water again, adding the adhesive, and repeating the process until the particle size of material particles in the ball rolling machine reaches 2.5mm, thus obtaining a first crude product;
(3) screening the first crude product in the step (2);
(4) adding the first coarse product screened in the step (3) into a ball rolling machine, controlling the rotating speed of the ball rolling machine to be 120r/min, rolling for 15min, and spraying 3% silica sol to the first coarse product while rolling the ball to obtain a second coarse product;
(5) putting the second crude product in the step (4) into a dryer to carry out five-section continuous drying, wherein the temperature of the first-section drying is controlled to be 80 ℃, the temperature of the second-section drying is controlled to be 90 ℃, the temperature of the third-section drying is controlled to be 100 ℃, the temperature of the fourth-section drying is controlled to be 110 ℃, the temperature of the fifth-section drying is controlled to be 120 ℃, and the water content of the second crude product after drying is controlled to be 30%;
(6) baking the second crude product dried in the step (5) in a rotary furnace, wherein the rotary furnace comprises six temperature zones, and the second crude product sequentially passes through a first temperature zone, a second temperature zone, a third temperature zone, a fourth temperature zone, a fifth temperature zone and a sixth temperature zone;
controlling the temperature of the first temperature zone to be 250 ℃, the temperature of the second temperature zone to be 300 ℃, the temperature of the third temperature zone to be 350 ℃, the temperature of the fourth temperature zone to be 450 ℃, the temperature of the fifth temperature zone to be 500 ℃, the temperature of the sixth temperature zone to be 550 ℃, and the total time of the second crude product passing through the six temperature zones to be 140min, thus obtaining a third crude product after the baking operation is finished;
(7) and (4) screening the third crude product in the step (6), standing and cooling to obtain the 4A molecular sieve.
Example 2
A4A molecular sieve was prepared according to the method of example 1, except that the raw materials used in the preparation were different in content, as shown in Table 1, and the rest was the same as in example 1.
The preparation method of the 4A molecular sieve comprises the following operation steps:
(1) uniformly mixing zeolite, carbon black, fumed silica and an adhesive to obtain a first mixture;
(2) adding the mixture I in the step (1) into a ball rolling machine, sprinkling water on the surface of the mixture I, adding an adhesive, controlling the rotating speed of the ball rolling machine to be 50r/min, rolling for 10min, then sprinkling water again and adding the adhesive, and repeating the process until the particle size of material particles in the ball rolling machine reaches 2mm, thus obtaining a first coarse product;
(3) screening the first crude product in the step (2);
(4) adding the first coarse product screened in the step (3) into a ball rolling machine, controlling the rotating speed of the ball rolling machine to be 30r/min for rolling for 10min, and spraying 3% silica sol to the first coarse product while performing ball rolling operation to obtain a second coarse product;
(5) putting the second crude product in the step (4) into a dryer to carry out five-stage continuous drying, wherein the temperature of the first-stage drying is controlled to be 60 ℃, the temperature of the second-stage drying is controlled to be 70 ℃, the temperature of the third-stage drying is controlled to be 80 ℃, the temperature of the fourth-stage drying is controlled to be 90 ℃, the temperature of the fifth-stage drying is controlled to be 100 ℃, and the water content of the second crude product after drying is controlled to be 30%;
(6) baking the second crude product dried in the step (5) in a rotary furnace, wherein the rotary furnace comprises six temperature zones, and the second crude product sequentially passes through a first temperature zone, a second temperature zone, a third temperature zone, a fourth temperature zone, a fifth temperature zone and a sixth temperature zone;
controlling the temperature of the first temperature zone to be 200 ℃, the temperature of the second temperature zone to be 250 ℃, the temperature of the third temperature zone to be 300 ℃, the temperature of the fourth temperature zone to be 400 ℃, the temperature of the fifth temperature zone to be 450 ℃, the temperature of the sixth temperature zone to be 500 ℃, and the total time of the second crude product passing through the six temperature zones to be 120min, and obtaining a third crude product after the baking operation is finished;
(7) and (4) screening the third crude product in the step (6), standing and cooling to obtain the 4A molecular sieve.
Example 3
A4A molecular sieve was prepared according to the method of example 1, except that the raw materials used in the preparation were different in content, as shown in Table 1, and the rest was the same as in example 1.
The preparation method of the 4A molecular sieve comprises the following operation steps:
(1) uniformly mixing zeolite, carbon black, fumed silica and an adhesive to obtain a first mixture;
(2) adding the mixture I in the step (1) into a ball rolling machine, sprinkling water on the surface of the mixture I, adding an adhesive, controlling the rotating speed of the ball rolling machine to be 100r/min, rolling for 15min, then sprinkling water again and adding the adhesive, and repeating the process until the particle size of material particles in the ball rolling machine reaches 2.3mm, thus obtaining a first crude product;
(3) screening the first crude product in the step (2);
(4) adding the first coarse product screened in the step (3) into a ball rolling machine, controlling the rotating speed of the ball rolling machine to be 75r/min, rolling for 13min, and spraying 3% silica sol to the first coarse product while rolling the ball to obtain a second coarse product;
(5) putting the second crude product in the step (4) into a dryer to carry out five-stage continuous drying, wherein the temperature of the first-stage drying is controlled to be 70 ℃, the temperature of the second-stage drying is controlled to be 80 ℃, the temperature of the third-stage drying is controlled to be 90 ℃, the temperature of the fourth-stage drying is controlled to be 100 ℃, the temperature of the fifth-stage drying is controlled to be 110 ℃, and the water content of the second crude product after drying is controlled to be 30%;
(6) baking the second crude product dried in the step (5) in a rotary furnace, wherein the rotary furnace comprises six temperature zones, and the second crude product sequentially passes through a first temperature zone, a second temperature zone, a third temperature zone, a fourth temperature zone, a fifth temperature zone and a sixth temperature zone;
the temperature of the first temperature zone is controlled to be 225 ℃, the temperature of the second temperature zone is controlled to be 275 ℃, the temperature of the third temperature zone is controlled to be 325 ℃, the temperature of the fourth temperature zone is controlled to be 425 ℃, the temperature of the fifth temperature zone is controlled to be 475 ℃, the temperature of the sixth temperature zone is controlled to be 525 ℃, the total time of the second crude product passing through the six temperature zones is 130min, and the third crude product is obtained after the baking operation is finished;
(7) and (4) screening the third crude product in the step (6), standing and cooling to obtain the 4A molecular sieve.
Example 4
A 4A molecular sieve which differs from example 3 in the amounts of starting materials used in its preparation, as shown in table 1, and is otherwise the same as in example 3.
Example 5
A 4A molecular sieve which differs from example 3 in the amounts of starting materials used in its preparation, as shown in table 1, and is otherwise the same as in example 3.
The preparation method of the 4A molecular sieve comprises the following operation steps:
(1) uniformly mixing zeolite, carbon black, fumed silica and an adhesive to obtain a first mixture;
(2) adding the mixture I in the step (1) into a ball rolling machine, sprinkling water on the surface of the mixture I, adding an adhesive, controlling the rotating speed of the ball rolling machine to be 100r/min, rolling for 15min, then sprinkling water again and adding the adhesive, and repeating the process until the particle size of material particles in the ball rolling machine reaches 2.3mm, thus obtaining a first crude product;
(3) screening the first crude product in the step (2);
(4) adding the first coarse product screened in the step (3) into a ball rolling machine, controlling the rotating speed of the ball rolling machine to be 75r/min, rolling for 13min, and spraying 4% silica sol to the first coarse product while rolling the ball to obtain a second coarse product;
(5) putting the second crude product in the step (4) into a dryer to carry out five-stage continuous drying, wherein the temperature of the first-stage drying is controlled to be 70 ℃, the temperature of the second-stage drying is controlled to be 80 ℃, the temperature of the third-stage drying is controlled to be 90 ℃, the temperature of the fourth-stage drying is controlled to be 100 ℃, the temperature of the fifth-stage drying is controlled to be 110 ℃, and the water content of the second crude product after drying is controlled to be 30%;
(6) baking the second crude product dried in the step (5) in a rotary furnace, wherein the rotary furnace comprises six temperature zones, and the second crude product sequentially passes through a first temperature zone, a second temperature zone, a third temperature zone, a fourth temperature zone, a fifth temperature zone and a sixth temperature zone;
the temperature of the first temperature zone is controlled to be 225 ℃, the temperature of the second temperature zone is controlled to be 275 ℃, the temperature of the third temperature zone is controlled to be 325 ℃, the temperature of the fourth temperature zone is controlled to be 425 ℃, the temperature of the fifth temperature zone is controlled to be 475 ℃, the temperature of the sixth temperature zone is controlled to be 525 ℃, the total time of the second crude product passing through the six temperature zones is 130min, and the third crude product is obtained after the baking operation is finished;
(7) and (4) screening the third crude product in the step (6), standing and cooling to obtain the 4A molecular sieve.
Example 6
A 4A molecular sieve which differs from example 3 in the amounts of starting materials used in its preparation, as shown in table 1, and is otherwise the same as in example 3.
Example 7
A 4A molecular sieve which differs from example 3 in the amounts of starting materials used in its preparation, as shown in table 1, and is otherwise the same as in example 3.
Example 8
A 4A molecular sieve which differs from example 3 in the amounts of starting materials used in its preparation, as shown in table 1, and is otherwise the same as in example 3.
The preparation method of the 4A molecular sieve comprises the following operation steps:
(1) uniformly mixing zeolite, carbon black, fumed silica and an adhesive to obtain a first mixture;
(2) adding the mixture I in the step (1) into a ball rolling machine, sprinkling water on the surface of the mixture I, adding an adhesive, controlling the rotating speed of the ball rolling machine to be 100r/min, rolling for 15min, then sprinkling water again and adding the adhesive, and repeating the process until the particle size of material particles in the ball rolling machine reaches 2.3mm, thus obtaining a first crude product;
(3) screening the first crude product in the step (2);
(4) adding the first coarse product screened in the step (3) into a ball rolling machine, controlling the rotating speed of the ball rolling machine to be 75r/min, rolling for 13min, and spraying 1% of silica sol to the first coarse product while rolling the ball to obtain a second coarse product;
(5) putting the second crude product in the step (4) into a dryer to carry out five-stage continuous drying, wherein the temperature of the first-stage drying is controlled to be 70 ℃, the temperature of the second-stage drying is controlled to be 80 ℃, the temperature of the third-stage drying is controlled to be 90 ℃, the temperature of the fourth-stage drying is controlled to be 100 ℃, the temperature of the fifth-stage drying is controlled to be 110 ℃, and the water content of the second crude product after drying is controlled to be 30%;
(6) baking the second crude product dried in the step (5) in a rotary furnace, wherein the rotary furnace comprises six temperature zones, and the second crude product sequentially passes through a first temperature zone, a second temperature zone, a third temperature zone, a fourth temperature zone, a fifth temperature zone and a sixth temperature zone;
the temperature of the first temperature zone is controlled to be 225 ℃, the temperature of the second temperature zone is controlled to be 275 ℃, the temperature of the third temperature zone is controlled to be 325 ℃, the temperature of the fourth temperature zone is controlled to be 425 ℃, the temperature of the fifth temperature zone is controlled to be 475 ℃, the temperature of the sixth temperature zone is controlled to be 525 ℃, the total time of the second crude product passing through the six temperature zones is 130min, and the third crude product is obtained after the baking operation is finished;
(7) and (4) screening the third crude product in the step (6), standing and cooling to obtain the 4A molecular sieve.
Example 9
A 4A molecular sieve which differs from example 3 in the amounts of starting materials used in its preparation, as shown in table 1, and is otherwise the same as in example 3.
The preparation method of the 4A molecular sieve comprises the following operation steps:
(1) uniformly mixing zeolite, carbon black, fumed silica and an adhesive to obtain a first mixture;
(2) adding the mixture I in the step (1) into a ball rolling machine, sprinkling water on the surface of the mixture I, adding an adhesive, controlling the rotating speed of the ball rolling machine to be 100r/min, rolling for 15min, then sprinkling water again and adding the adhesive, and repeating the process until the particle size of material particles in the ball rolling machine reaches 2.3mm, thus obtaining a first crude product;
(3) screening the first crude product in the step (2);
(4) adding the first coarse product screened in the step (3) into a ball rolling machine, controlling the rotating speed of the ball rolling machine to be 75r/min, rolling for 13min, and spraying 5% silica sol to the first coarse product while rolling the ball to obtain a second coarse product;
(5) putting the second crude product in the step (4) into a dryer to carry out five-stage continuous drying, wherein the temperature of the first-stage drying is controlled to be 70 ℃, the temperature of the second-stage drying is controlled to be 80 ℃, the temperature of the third-stage drying is controlled to be 90 ℃, the temperature of the fourth-stage drying is controlled to be 100 ℃, the temperature of the fifth-stage drying is controlled to be 110 ℃, and the water content of the second crude product after drying is controlled to be 30%;
(6) baking the second crude product dried in the step (5) in a rotary furnace, wherein the rotary furnace comprises six temperature zones, and the second crude product sequentially passes through a first temperature zone, a second temperature zone, a third temperature zone, a fourth temperature zone, a fifth temperature zone and a sixth temperature zone;
the temperature of the first temperature zone is controlled to be 225 ℃, the temperature of the second temperature zone is controlled to be 275 ℃, the temperature of the third temperature zone is controlled to be 325 ℃, the temperature of the fourth temperature zone is controlled to be 425 ℃, the temperature of the fifth temperature zone is controlled to be 475 ℃, the temperature of the sixth temperature zone is controlled to be 525 ℃, the total time of the second crude product passing through the six temperature zones is 130min, and the third crude product is obtained after the baking operation is finished;
(7) and (4) screening the third crude product in the step (6), standing and cooling to obtain the 4A molecular sieve.
Example 10
A 4A molecular sieve which differs from example 3 in the amounts of starting materials used in its preparation, as shown in table 1, and is otherwise the same as in example 3.
The preparation method of the 4A molecular sieve comprises the following operation steps:
(1) uniformly mixing zeolite, carbon black, fumed silica and an adhesive to obtain a first mixture;
(2) adding the mixture I in the step (1) into a ball rolling machine, sprinkling water on the surface of the mixture I, adding an adhesive, controlling the rotating speed of the ball rolling machine to be 100r/min, rolling for 15min, then sprinkling water again and adding the adhesive, and repeating the process until the particle size of material particles in the ball rolling machine reaches 2.3mm, thus obtaining a first crude product;
(3) screening the first crude product in the step (2);
(4) adding the first coarse product screened in the step (3) into a ball rolling machine, controlling the rotating speed of the ball rolling machine to be 75r/min, rolling for 13min, and spraying 4% silica sol to the first coarse product while rolling the ball to obtain a second coarse product;
(5) putting the second crude product in the step (4) into a dryer to carry out five-stage continuous drying, wherein the temperature of the first-stage drying is controlled to be 70 ℃, the temperature of the second-stage drying is controlled to be 80 ℃, the temperature of the third-stage drying is controlled to be 90 ℃, the temperature of the fourth-stage drying is controlled to be 100 ℃, the temperature of the fifth-stage drying is controlled to be 110 ℃, and the water content of the second crude product after drying is controlled to be 30%;
(6) baking the second crude product dried in the step (5) in a rotary furnace, wherein the rotary furnace comprises six temperature zones, and the second crude product sequentially passes through a first temperature zone, a second temperature zone, a third temperature zone, a fourth temperature zone, a fifth temperature zone and a sixth temperature zone;
the temperature of the first temperature zone is controlled to be 225 ℃, the temperature of the second temperature zone is controlled to be 275 ℃, the temperature of the third temperature zone is controlled to be 325 ℃, the temperature of the fourth temperature zone is controlled to be 425 ℃, the temperature of the fifth temperature zone is controlled to be 475 ℃, the temperature of the sixth temperature zone is controlled to be 525 ℃, the total time of the second crude product passing through the six temperature zones is 130min, and the third crude product is obtained after the baking operation is finished;
(7) and (4) screening the third crude product in the step (6), standing and cooling to obtain the 4A molecular sieve.
TABLE 1
The raw materials and contents in the examples of the present application are shown in table 1.
Comparative example
Comparative example 1
A 4A molecular sieve which differs from example 3 in that the starting material used in its preparation does not contain carbon black, and is otherwise the same as in example 3.
The preparation method of the 4A molecular sieve is different from the preparation method of the example 3 in that no carbon black is contained in the step (1), and the rest is the same as the preparation method of the example 3.
Comparative example 2
A 4A molecular sieve which differs from example 3 in that the starting material used in its preparation does not contain fumed silica, and is otherwise the same as in example 3.
The preparation method of the 4A molecular sieve is different from the preparation method of the example 3 in that the step (1) does not contain fumed silica, and the rest is the same as the step (3).
Comparative example 3
A 4A molecular sieve which differs from example 3 in that the starting materials used in its preparation do not contain fumed silica and carbon black, and is otherwise the same as in example 3.
The preparation method of the 4A molecular sieve is different from the preparation method of the example 3 in that the fumed silica and the carbon black are not contained in the step (1), and the rest is the same as the step (3).
Comparative example 4
A 4A molecular sieve which differs from example 3 in that it is prepared in a process which does not include silica sol in step (4), otherwise the same as in example 3.
Performance testing test subjects: the 4A molecular sieves prepared in examples 1-10 were used as test samples 1-10, and the 4A molecular sieves prepared in comparative examples 1-4 were used as comparative samples 1-4, and the total number of groups was 14, and each group had 30 small samples.
1. Static water adsorption Properties
And (4) according to GB/T6287, carrying out static water adsorption performance detection on the test samples 1-10 and the comparison samples 1-4.
TABLE 2
The results of the static water adsorption test are shown in table 2 above.
It can be seen from the combination of examples 1 to 10 and comparative examples 1 to 4 and the combination of table 2 that the 4A molecular sieves prepared in examples 1 to 10 have good adsorption performance, and the 4A molecular sieves prepared in examples 1 to 10 and comparative examples 2 and 4 have higher adsorption capacity than the 4A molecular sieves prepared in comparative examples 1 and 3, so that the adsorption capacity of the 4A molecular sieve can be improved by adding carbon black.
2. Wear rate detection
The test samples 1 to 10 and the comparative samples 1 to 4 were subjected to wear rate detection according to GB 10505.2-1989.
TABLE 3
| Sample (I) | Abrasion Rate (%) |
| Test sample 1 | 0.34 |
| Test sample 2 | 0.25 |
| Test sample 3 | 0.26 |
| Test sample 4 | 0.28 |
| Test sample 5 | 0.33 |
| Test sample 6 | 0.22 |
| Test sample 7 | 0.35 |
| Test specimen 8 | 0.30 |
| Test sample 9 | 0.23 |
| Test specimen 10 | 0.24 |
| Comparative sample 1 | 0.74 |
| Comparative sample 2 | 0.71 |
| Comparative sample 3 | 0.85 |
| Comparative sample 4 | 0.65 |
The results of the abrasion rate test are shown in table 3 above.
It can be seen by combining examples 1 to 10 with comparative example 4 and combining table 3 that the abrasion rates of the test samples 1 to 10 are lower than that of the comparative sample 4, so that the addition of silica sol in the step (4) of the preparation operation can significantly reduce the abrasion rate of the 4A molecular sieve and improve the wear resistance of the 4A molecular sieve.
By combining examples 1-10 with comparative examples 1-3 and table 3, it can be seen that the abrasion rates of the test samples 1-10 are lower than those of the comparative samples 1-3, and therefore, the addition of carbon black and fumed silica can significantly reduce the abrasion rate of the 4A molecular sieve and improve the abrasion resistance of the 4A molecular sieve.
As can be seen from the combination of examples 3, 9 to 10 and example 8 and Table 3, the abrasion ratios of the test samples 3, 9 to 10 were lower than that of the test sample 8, and therefore the appropriate amount of silica sol to be added was 3 to 5%.
In the combination of examples 2, 3, 6, 8 to 10 and examples 1, 4, 5 and 7 and in Table 3, it can be seen that the abrasion ratios of the test samples 2, 3, 6, 8 to 10 were lower than those of the test samples 1, 4, 5 and 7, and therefore the appropriate amount of carbon black to be added was 3 to 5%.
In combination with examples 2, 3, 6, 8 to 10 and examples 1, 4, 5 and 7 and in combination with table 3, it can be seen that the abrasion ratios of the test samples 2, 3, 6, 8 to 10 are lower than the abrasion ratios of the test samples 1, 4, 5 and 7, and therefore the appropriate amount of addition of fumed silica is 12 to 16%.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (8)
1. The 4A molecular sieve is characterized in that the 4A molecular sieve is prepared from the following raw materials in percentage by mass:
57-67% of zeolite
20 percent of adhesive
1 to 5 percent of carbon black
8-16% of fumed silica
The zeolite is a 4A zeolite.
2. The 4A molecular sieve of claim 1, characterized in that: the adhesive is formed by combining one or two of attapulgite and kaolin.
3. The 4A molecular sieve of claim 2, characterized in that: the adhesive is composed of attapulgite and kaolin, wherein the attapulgite accounts for 5-15% of the mass of the 4A molecular sieve, and the kaolin accounts for 5-15% of the mass of the 4A molecular sieve.
4. The 4A molecular sieve of claim 1, characterized in that: the mass percentage of the carbon black is 3-5%.
5. The 4A molecular sieve of claim 1, characterized in that: the mass percentage of the fumed silica is 12-16%.
6. A process for the preparation of a 4A molecular sieve as claimed in any one of claims 1 to 5, comprising the steps of:
(1) uniformly mixing zeolite, carbon black, fumed silica and an adhesive to obtain a first mixture;
(2) adding the mixture I in the step (1) into a ball rolling machine, spraying water on the surface of the mixture I, adding an adhesive, controlling the rotating speed of the ball rolling machine to be 50-150 r/min, rolling for 10-20 min, then spraying water again, adding the adhesive, and repeating the process until the particle size of material particles in the ball rolling machine reaches 2-2.5 mm, so as to obtain a first coarse product;
(3) screening the first crude product in the step (2);
(4) adding the first coarse product screened in the step (3) into a ball rolling machine, controlling the rotating speed of the ball rolling machine to be 30-120 r/min, rolling for 10-15 min, and spraying silica sol to the first coarse product while rolling the ball to obtain a second coarse product;
(5) putting the second crude product in the step (4) into a dryer to carry out five-stage continuous drying, wherein the temperature of the first-stage drying is controlled to be 60-80 ℃, the temperature of the second-stage drying is controlled to be 70-90 ℃, the temperature of the third-stage drying is controlled to be 80-100 ℃, the temperature of the fourth-stage drying is controlled to be 90-110 ℃, the temperature of the fifth-stage drying is controlled to be 100-120 ℃, and the water content of the second crude product after drying is controlled to be 30%;
(6) baking the second crude product dried in the step (5) in a rotary furnace, wherein the rotary furnace comprises six temperature zones, and the second crude product sequentially passes through a first temperature zone, a second temperature zone, a third temperature zone, a fourth temperature zone, a fifth temperature zone and a sixth temperature zone;
controlling the temperature of the first temperature zone to be 200-250 ℃, the temperature of the second temperature zone to be 250-300 ℃, the temperature of the third temperature zone to be 300-350 ℃, the temperature of the fourth temperature zone to be 400-450 ℃, the temperature of the fifth temperature zone to be 450-500 ℃, the temperature of the sixth temperature zone to be 500-550 ℃, and the total time of the second crude product passing through the six temperature zones to be 120-140 min, and finishing the baking operation to obtain a third crude product;
(7) and (4) screening the third crude product in the step (6), standing and cooling to obtain the 4A molecular sieve.
7. The method of preparing a 4A molecular sieve of claim 6, characterized in that: the mass percentage of the added silica sol in the step (4) is 1-5%.
8. The method of preparing a 4A molecular sieve of claim 7, characterized in that: the mass percentage of the added silica sol in the step (4) is 3-5%.
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| CN114669276A (en) * | 2022-02-16 | 2022-06-28 | 杭州远烨新材料有限公司 | Production process of molecular sieve desiccant |
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